反应 #1730586

ord-21410723ac3d41d79c7a9d1c12d582a3

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤filtered
  2. 2
    浓缩concentrated
  3. 3
    workup.DISSOLUTIONThe residue was redissolved in DCM/n-hexane
  4. 4
    浓缩concentrated under reduced pressure
  5. 5
    其他The crude oil was purified by flash chromatography (Biotage SP1, EtOAc/n-hexane from 5 to 10%)

实验过程

To a solution of 5-hexenoic acid (15.2 mL, 0.131 mol) in DCM (375 mL), cooled to 0° C., tert-butanol (176 mL, 1.84 mol) and then 4-dimethylaminopyridine (3.21 g, 26.3 mmol) were added. The mixture was stirred at room temperature for 22 hrs, filtered and concentrated. The residue was redissolved in DCM/n-hexane and concentrated under reduced pressure. The crude oil was purified by flash chromatography (Biotage SP1, EtOAc/n-hexane from 5 to 10%), affording the title product.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08119806B2uspto-grants-2012_02